CN1990426A - Aluminum nitride bonded body, and manufacturing method of the same - Google Patents
Aluminum nitride bonded body, and manufacturing method of the same Download PDFInfo
- Publication number
- CN1990426A CN1990426A CNA2006101714108A CN200610171410A CN1990426A CN 1990426 A CN1990426 A CN 1990426A CN A2006101714108 A CNA2006101714108 A CN A2006101714108A CN 200610171410 A CN200610171410 A CN 200610171410A CN 1990426 A CN1990426 A CN 1990426A
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- China
- Prior art keywords
- aluminum nitride
- fixing body
- weight
- knitting layer
- aluminium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical group Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 63
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000009940 knitting Methods 0.000 claims description 52
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 40
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 37
- 229910017083 AlN Inorganic materials 0.000 claims description 34
- 239000011575 calcium Substances 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 230000004907 flux Effects 0.000 claims description 25
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 20
- 229910052791 calcium Inorganic materials 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 13
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 12
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000292 calcium oxide Substances 0.000 claims description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 230000003746 surface roughness Effects 0.000 claims description 9
- 239000004411 aluminium Substances 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 21
- 239000000203 mixture Substances 0.000 description 12
- 230000002093 peripheral effect Effects 0.000 description 11
- 239000001307 helium Substances 0.000 description 9
- 229910052734 helium Inorganic materials 0.000 description 9
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 9
- 239000007790 solid phase Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000000465 moulding Methods 0.000 description 7
- 238000005304 joining Methods 0.000 description 5
- 229910052727 yttrium Inorganic materials 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000005382 thermal cycling Methods 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 229910052772 Samarium Inorganic materials 0.000 description 3
- 229910052769 Ytterbium Inorganic materials 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011499 joint compound Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-OUBTZVSYSA-N Ammonia-15N Chemical compound [15NH3] QGZKDVFQNNGYKY-OUBTZVSYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- C04B2237/32—Ceramic
- C04B2237/36—Non-oxidic
- C04B2237/366—Aluminium nitride
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/62—Forming laminates or joined articles comprising holes, channels or other types of openings
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/80—Joining the largest surface of one substrate with a smaller surface of the other substrate, e.g. butt joining or forming a T-joint
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Abstract
The present invention provided an aluminum nitride bonded body which can receive a good bonding state even under the lower bonding temperature and do not need bringing the pressure in the manufacture procedure and the manufacture method thereof. The aluminum nitride bonded body includes: a stick-like attaching body containing aluminum nitride; an attached body containing aluminum nitride, in which a tip end portion of the attaching body is screwed to a support hole; and a bonding layer for bonding the attaching body and the attached body to each other.
Description
Technical field
The present invention relates to aluminium nitride and manufacture method thereof, more specifically relate to conjugant and manufacture method thereof as a plurality of aluminium nitride components bonding of the component parts of semiconductor-fabricating device.
Background technology
In the past, under the situation that makes the aluminium nitride components bonding, for example using sometimes, solid phase engaged.It is not have grafting material and the method (for example, with reference to patent documentation 1 " spy opens flat 8-73280 communique ") that engages under solid state shape between the aluminium nitride parts that solid phase engages.
In addition, currently known methods is, between a plurality of basic materials that aluminium nitride matter pottery is constituted, setting contains the joint compound of aluminium nitride matter pottery and flux, then, applied load is made conjugant (for example, with reference to patent documentation 2 " No. 3604888 communiques of patent ") when being heated to preset temperature.
Use these joining techniques, make as formation and have the heating unit of heating element and have the semiconductor-fabricating device of parts of the electrostatic chuck etc. of electrode.
But, in above-mentioned existing solid phase engages, for obtaining good engagement state, and junction temperature need be set at the high temperature more than 1850 ℃, so the aluminium nitride parts might be out of shape because of joint.
In addition, carry out in the manufacturing engineering of heating unit and electrostatic chuck under the situation of solid phase joint, by high junction temperature, it is rotten heating element and electrode to occur, or volume specific resistance changes.Its result, the possibility that has the even heating decline of heating unit and cause the adsorptive power of electrostatic chuck to descend.In addition, owing to need the planeness on extraordinary junction surface, thus not only become the major reason that cost increases, but also limited the shape at junction surface.
Have again, in above-mentioned patent documentation 2 in the disclosed method of joining, as described in the specification sheets the 0061st section, in heating basic material and joint compound, sometimes need with the orthogonal direction in junction surface on pressurize.
Summary of the invention
So, also can obtain good engagement state even the purpose of this invention is to provide under low junction temperature, and not need the aluminum nitride bonded body and the manufacture method thereof of pressurizeing in the manufacturing process.
For achieving the above object, aluminum nitride bonded body of the present invention is characterized in that, possesses: the bar-shaped fixing body that comprises aluminium nitride; Comprise aluminium nitride, and the leading section of above-mentioned fixing body is threaded onto the body that is mounted in the supported hole; At these fixing bodies and being mounted in the contact part of body, be formed on fixing body at least and bear the pressure contact portion of crimp force, and make above-mentioned fixing body and be mounted the knitting layer that body engages by above-mentioned being threaded; This knitting layer comprises nitrogen, oxygen, aluminium, calcium, and the amount of rare earth element is discontented with 15 weight %.
In the past, will contain the fixing body of aluminium nitride and to be mounted the method that body engages mainly be that solid phase engages and the liquid phase joint.In addition, for No. 3604888 communique of above-mentioned Japan patent (patent documentation 2), as illustrating, owing to needed the operation of pressurizeing in the past, be mounted on the body so be difficult to a plurality of fixing bodies are joined to simultaneously.But,, be mounted on the body owing to a plurality of fixing bodies are joined to simultaneously, so can improve manufacturing efficient according to the present invention.
In addition, for carefully bar-shaped, for example be under elongate cylindrical shape and the situation cylindraceous at fixing body, be difficult to push fixing body to being mounted the body applied load in the past.But according to the present invention, fixing body and being mounted in the contact part of body forms knitting layer at fixing body on by the above-mentioned pressure contact portion that bears crimp force that is threaded at least.That is,, do not need to make aluminum nitride bonded body efficiently to fixing body applied load and pushing owing to utilize the crimp force that is produced that is threaded to engage.
In addition, because above-mentioned grafting material comprises aluminium nitride, so, can reliably fixing body be joined to and be mounted on the body to aluminium nitride connectivity height.
Have again, above-mentioned fixing body and being mounted in the contact part of body, at least knitting layer is set at fixing body on by the above-mentioned pressure contact portion that bears crimp force that is threaded, even so be under the big situation of the surfaceness of pressure contact portion at the position that knitting layer is set, knitting layer enters in form on this junction surface small concavo-convex, also can guarantee fixing body joined to be mounted on the body.
Above-mentioned knitting layer it is desirable to comprise 15～30 weight % nitrogen, 10～35 weight % oxygen, 20～55 weight % aluminium, 5～20 weight % calcium.
It is desirable to, above-mentioned fixing body is formed inside have the cylindric of through hole, simultaneously, by above-mentioned be mounted on the body to form be communicated to the patchhole of supported hole bottom surface, and the through hole of fixing body is communicated to above-mentioned the inserting in the hole of body that be mounted.
Because the inner through hole that forms of fixing body is communicated with the patchhole that is mounted body, so can carry fluids such as helium to being mounted body from fixing body.In addition, by above-mentioned grafting material, can seal the leading section of supported hole and fixing body reliably.
Above-mentioned fixing body and be mounted body and can under 300 ℃～800 ℃ the condition of high temperature, use.
The above-mentioned body that is mounted is the heating unit that constitutes semiconductor-fabricating device, and the fixing body ideal is a tubular part.
In addition, owing to can engage at low temperatures with existing method of joining comparison, so the heating element of the heating unit of semiconductor-fabricating device never degenerates, and volume specific resistance is also almost constant when engaging, so as heating unit performance premium properties.
The manufacture method of aluminum nitride bonded body of the present invention has following steps: in the bar-shaped fixing body that contains aluminium nitride and the step of smearing grafting material at least one of body that is mounted that contains aluminium nitride; Described fixing body is threaded onto in the supported hole that is mounted body, and described fixing body is crimped onto the step that is mounted on the body by described grafting material; And by to described fixing body, grafting material and be mounted body and heat with the junction temperature below 1500 ℃, fixing body is situated between is bonded on the step that is mounted on the body by knitting layer,
Described grafting material contains calcium aluminium oxide or calcium oxide and aluminum oxide by comprising, and the flux and the aluminium nitride powder that contain the discontented 5 weight % of rare earth element, and with fixing body be mounted in the contact part of body at least because of above-mentioned being threaded makes fixing body bear pressure contact portion from the crimp force that is mounted body, be bonded with each other by knitting layer.
According to this type of manufacture method, owing to the low temperature that junction temperature is set at below 1500 ℃, the thermal distortion of aluminum nitride bonded body in the time of can significantly reducing to engage.In addition, because junction temperature is low, thus can reduce to engage required energy, and the reprocessing after engaging do not need yet, so can significantly reduce manufacturing cost.
In above-mentioned manufacture method, it is desirable to rise to above-mentioned junction temperature for 0.5～10.0 ℃/minute with heat-up rate.
Above-mentioned fixing body and being mounted in the contact part of body it is desirable to, and the average surface roughness because of the above-mentioned pressure contact portion that bears crimp force of being threaded is 0.4～1.6 μ m at least.
By adopting this average surface roughness, form on the above-mentioned pressure contact portion surface concavo-convex filled up in grafting material fusing or softening, so can improve fixing body and the bond strength that is mounted body.
According to aluminum nitride bonded body of the present invention and manufacture method, a plurality of fixing bodies can be joined to simultaneously and be mounted on the body.In the past, will contain the fixing body of aluminium nitride and to be mounted the method that body engages mainly be that solid phase engages and the liquid phase joint.In addition, because as the explanation of No. 3604888 communique of above-mentioned Japanese Patent is needed the operation of pressurizeing in the past ceramic indirect fashionable, be mounted on the body so be difficult to a plurality of fixing bodies are joined to simultaneously.But,, a plurality of fixing bodies can be joined to simultaneously and be mounted on the body according to the present invention.
In addition, according to the manufacture method of aluminum nitride bonded body of the present invention, owing to the low temperature that junction temperature is set at below 1500 ℃, so can significantly reduce the thermal distortion of aluminum nitride bonded body when engaging.And, owing to when engaging, do not need fixing body being mounted the body pressurization, so can reduce worker the time.
Description of drawings
Fig. 1 is the sectional view of the aluminum nitride bonded body of expression embodiment of the present invention.
Fig. 2 is the sectional view of the aluminum nitride bonded body of another embodiment of expression the present invention.
Fig. 3 is the sectional view of heating unit of the semiconductor-fabricating device of expression embodiment of the present invention.
Fig. 4 is the sectional view of the aluminum nitride bonded body of the another embodiment of expression the present invention.
Fig. 5 is the sectional view of the aluminum nitride bonded body of the another embodiment of expression the present invention.
Fig. 6 is the sectional view of the aluminum nitride bonded body of the another embodiment of expression the present invention.
Fig. 7 is the sectional view of the aluminum nitride bonded body of the another embodiment of expression the present invention.
Fig. 8 is the sectional view of the aluminum nitride bonded body of the another embodiment of expression the present invention.
Among the figure:
1,21-aluminum nitride bonded body, 3,23,52,82-fixing body, 3a, 23a-leading section, 5,25, the 56-supported hole, 7,27,53,62,83-is mounted body, 11,44,57-knitting layer, 31,86-through hole, 33-patchhole, 41-heating unit, 42-disc-shaped part (being mounted body), 43-tubular part (fixing body)
Embodiment
Aluminum nitride bonded body and manufacture method thereof to embodiment of the present invention describes below.
(grafting material)
The grafting material of embodiment of the present invention comprises flux and aluminium nitride (AlN) powder, applicable to the fixing body that comprises aluminium nitride and be mounted body joint each other.
Grafting material it is desirable to contain 10～90 weight % flux, 10～90 weight % aluminium nitride powders.According to the cooperation of this type of flux and aluminium nitride powder, can reduce to contain the fixing body of aluminium nitride and be mounted body and the thermal expansion difference of grafting material, and can be in the bonding part residual an amount of flux.Therefore, can improve the intensity and the resistance to air loss of bonding part.What grafting material was better is to contain 80～40 weight % flux, 20～60 weight % aluminium nitride powders.Have again, also can contain Y, Yb, the such rare earth element of Sm, Ce in the aluminium nitride powder.
(flux)
Flux contains calcium aluminium oxide (CaxAlyOz), or calcium oxide (CaO) and aluminum oxide (Al
2O
3).That is, flux contains calcium aluminium oxide at least, or calcium oxide and aluminum oxide both.Therefore, flux it is desirable to only to contain calcium aluminium oxide, contains calcium aluminium oxide and calcium oxide, contains calcium aluminium oxide and aluminum oxide, contains calcium aluminium oxide and calcium oxide and aluminum oxide, contains calcium oxide and aluminum oxide.
In addition, as calcium aluminium oxide (CaxAlyOz), flux can contain Ca
12Al
14O
33(x=12, y=14, z=33) or Ca
3Al
2O
6At least a in (x=3, y=2, z=6).That is, as calcium aluminium oxide, flux can only contain Ca
12Al
14O
33, also can only contain Ca
3Al
2O
6, also can contain Ca
12Al
14O
33And Ca
3Al
2O
6Both remove Ca
12Al
14O
33And Ca
3Al
2O
6Outside, also can contain Ca
12Al
14O
33And Ca
3Al
2O
6Calcium aluminium oxide with the foreign minister.Have, the content of the rare earth element in the flux (Y, Yb, Sm, Ce) is with respect to the discontented 5 weight % (corresponding to the record of scheme 4) of flux entire amount again.Also have, also can be fully rear earth containing element not.
(aluminum nitride bonded body)
As shown in Figure 1, the aluminum nitride bonded body 1 of present embodiment possesses elongate cylindrical shape of forming (bar-shaped) is the fixing body 3 of principal constituent with the aluminium nitride, the leading section 3a of fixing body 3 to be threaded and to join in the supported hole 5 be the knitting layer 11 that is mounted body 7, disposes on the whole in the bottom surface 9 of the supported hole 5 that is mounted body 7 of principal constituent with the aluminium nitride.This knitting layer 11 contains nitrogen (N), oxygen (O), aluminium (Al), calcium (Ca), the amount less than 15 weight % of rare earth element.Have, rare earth element contained in the knitting layer 11 is contained in the grafting material originally again, and, as the fixing body 3 that is engaged object be mounted that contained rare earth element enters in the knitting layer 11 in the aluminium nitride in the body 7.In addition, also can be fully rear earth containing element not.
Because this type of aluminum nitride bonded body 1 can obtain by the low junction temperature below 1500 ℃, thus the fixing body 3 can suppress to engage the time and be mounted the thermal distortion of body 7, and engagement state is also good.In addition, engage fixing body 3 front end face 3b and the bottom surface 9 that is mounted the supported hole 5 of body 7 by knitting layer 11.This fixing body 3 is being threaded onto under the state of the supported hole 5 that is mounted body 7,9 knitting layer 11 bears the crimp force that is threaded and is produced to the front end face 3b of fixing body 3 from the bottom surface.Like this, in the aluminum nitride bonded body of Fig. 1, the bottom surface 9 of front end face 3b and supported hole 5 becomes pressure contact portion.Therefore, so applied load as in the past not, and can utilize the crimp force that is produced that is threaded to engage is can reduce the worker of conjugant the time.Fixing body 3 and the material that is mounted body 7 are principal constituent with the aluminium nitride, can contain (Y, Yb, Sm, Ce) such rare earth element.
Have, knitting layer 11 it is desirable to contain 15～30 weight % nitrogen, 10～35 weight % oxygen, 20～55 weight % aluminium, 5～20 weight % calcium again.By the composition of this type of knitting layer 11, can improve the intensity and the resistance to air loss of bonding part.Knitting layer 11 it is desirable to contain for example compound N-O-Al-Ca and compound N-O-Al-Ca-X (X is a rare earth element), calcium oxide, aluminum oxide, calcium aluminium oxide etc.
As shown in Figure 2, another aluminum nitride bonded body 21 of present embodiment possesses the fixing body 23 of elongate cylindrical shape of forming (bar-shaped), the leading section 23a of fixing body 23 is threaded and joins to the knitting layer 11 that is mounted body 27, disposes on the whole in the bottom surface 29 of the supported hole 25 that is mounted body 27 in the supported hole 25.This knitting layer 11 contains and the above-mentioned identical composition of knitting layer illustrated in fig. 1.Because this type of aluminum nitride bonded body 21 can obtain by the low junction temperature below 1500 ℃, thus the fixing body 23 can suppress to engage the time and be mounted the thermal distortion of body 27, and engagement state is also good.In addition, because applied load as in the past not, and can utilize the crimp force that is produced that is threaded to engage, so can reduce the worker of conjugant the time.
In addition, fixing body 23 forms the general cylindrical shape that inside has through hole 31.Be mounted and formed supported hole 25 on the body 27, formed the patchhole 33 that is communicated with bottom surface 29 in this supported hole 25.Therefore, constitute, patchhole 33 and through hole 31 interconnect, so when importing fluid such as helium from the front end of fixing body 23, this fluid is transported to patchhole 33 from through hole 31.
Fig. 3 is the sectional view of heating unit of the semiconductor-fabricating device of expression embodiment of the present invention.This heating unit 41 possesses as the disc-shaped part (dish) 42 that is mounted body, as the tubular part (axle) 43 of fixing body, with the knitting layer 44 of these disc-shaped parts 42 and tubular part 43 joints, and disc-shaped part 42 and tubular part 43 all contain aluminium nitride.
Buried heating element 45 underground in the inside of disc-shaped part 42.As this heating element 45, can use molybdenum (Mo), tungsten (W) constant resistance heating element.In addition, heating element 45 can use shapes such as wire, coiled type, mesh-like, sheet, bulk.
Be the loading surface 42a that has loaded semiconductor substrate (wafer) above the disc-shaped part 42, engaged tubular part 43 on the opposite side back side 42b of this loading surface 42a.Specifically, formed circular recess (supported hole) 46 on the 42b of the back side, formed knitting layer 11 at the inner face of this recess 46.And the front end 43a of tubular part 43 embeds in the recess 46, and this front end 43a embeds and joins in the recess 46 by above-mentioned knitting layer 11.Even in this case, because applied load as in the past not, and can utilize the crimp force that is produced that is threaded to engage, so also can reduce the worker of conjugant the time.In addition, this knitting layer 11 contains and above-mentioned Fig. 1 and the identical composition of knitting layer illustrated in fig. 2.
In addition, in interior all sides of tubular part 43, held power supply part 47 cylindraceous, the end 47a of power supply part 47 waits by welding and is electrically connected with the terminal of heating element 45.Like this, power supply part 47 can be to heating element 45 supply capabilities.
In addition, for other aluminum nitride bonded body of present embodiment, use Fig. 4～Fig. 8 to describe.
These aluminum nitride bonded bodies 51,61,71,81,91, be threaded as the bolt 52,82 of fixing body with respect to the body 53,62,83 that is mounted with the supported hole 56 that runs through, simultaneously, at bolt 52,82 be mounted on the contact part between the body 53,62,83 and formed knitting layer 57.Specify below.
Aluminum nitride bonded body 51 shown in Figure 4 possesses bolt 52 as fixing body, have supported hole 56 be mounted body 53 and at bolt 52 be mounted the knitting layer 11 that the contact part of body 53 forms.
Bolt 52 is by head 54 and bolt part 55 integrated formation that are provided with in this head 54 bottoms, and this bolt part 55 is threaded onto in the bolt hole 56 that is mounted body 53.In addition, by being threaded of bolt 52, below the peripheral part of the head 54 of bolt 52 58 bear from be mounted body 53 above 59 crimp forces that make progress.Like this, 58 and top 59 become pressure contact portion below the peripheral part.
And, knitting layer 11 be formed at below the peripheral part of bolt 52 58 and be mounted body 53 top 59 between, and the periphery of the bolt part 55 of bolt 52 and being mounted between the inner peripheral surface of bolt hole 56 of body 53.This knitting layer 11 also has and above-mentioned Fig. 1～identical composition of knitting layer illustrated in fig. 3.
Then, in aluminum nitride bonded body shown in Figure 5 61, be mounted and formed gap 64 above the body 62, disposed the head 54 of bolt 52 in this gap 64.
Even in this case, by being threaded of bolt 52,58 bear above the gap 64 that is mounted body 62 59 upward crimp forces below the peripheral part of the head 54 of bolt 52.Like this, below the peripheral part 58 and above 59 become pressure contact portion.Knitting layer 11 be formed at as below the peripheral part of bolt 52 58 and be mounted body 62 gap 64 top 59 between, and the periphery of the bolt part 55 of bolt 52 and being mounted between the inner peripheral surface of bolt hole 56 of body 62.This knitting layer 11 also has and above-mentioned Fig. 1～identical composition of knitting layer illustrated in fig. 4.
Aluminum nitride bonded body 71 shown in Figure 6 possesses bolt 52 and is mounted body 53 and knitting layer 57.With Fig. 4 relatively, this situation does not form knitting layer on bolt part 55, below the peripheral part of the head 54 of bolt 52 58 and be mounted body 53 top 59 between formed knitting layer 11.Like this, below the peripheral part 58 and above 59 become pressure contact portion.This knitting layer 11 also has and above-mentioned Fig. 1～identical composition of knitting layer illustrated in fig. 5.
In addition, Fig. 7 and aluminum nitride bonded body 81,91 shown in Figure 8 are provided with the through hole 86 that runs through vertically on bolt 82.
That is, aluminum nitride bonded body 81 shown in Figure 7 is the formation identical substantially with the aluminum nitride bonded body 51 of Fig. 4, but has formed difference on through hole 86 these aspects vertically in the radial center portion as the bolt 82 of fixing body.In addition, aluminum nitride bonded body 91 shown in Figure 8 is the formation identical substantially with the aluminum nitride bonded body 71 of Fig. 6, but has formed difference on through hole 86 these aspects vertically in the radial center portion as the bolt 82 of fixing body.Even in these aluminum nitride bonded bodies 81,91, by being threaded of bolt 82, below the peripheral part of the head 84 of bolt 82 58 bear from be mounted body 83 above 59 upward crimp forces.Therefore, because applied load as in the past not, and can utilize the crimp force that is produced that is threaded to engage, so also can reduce the worker of conjugant the time.Have, Fig. 7,8 knitting layer 11 also contain and above-mentioned Fig. 1～identical composition of knitting layer illustrated in fig. 6 again.
According to these aluminum nitride bonded bodies 51,61,81,91, bolt hole 56 runs through on the thickness direction that is mounted body 53,62,83, so can reduce to be mounted the thickness of body 53,62,83.
(manufacture method of aluminum nitride bonded body)
Manufacture method for the aluminum nitride bonded body of embodiment of the present invention describes with reference to Fig. 2.
(grafting material smear operation)
On the side of the supported hole 25 that is mounted body 27, cut negative thread.At first, near 29 sides smear grafting material from the bottom surface 29 of supported hole 25 to the bottom surface.In addition, the average surface roughness of the bottom surface 29 of supported hole 25 is 0.4～1.6 μ m.
This grafting material contains calcium aluminium oxide or calcium oxide and aluminum oxide, and contains flux and the aluminium nitride powder of rare-earth-type material less than 5 weight %.In addition, for being easy to smear, grafting material can mix use IPA (Virahol), ethanol etc.In addition, also grafting material can be formed sheet, be disposed at the bottom surface 29 of supported hole 25, be clipped in fixing body 23 and be mounted between the body 27.Even for the quantitative change that makes grafting material, it is desirable to 5～35mg/cm
2The amount of better grafting material is 10～30mg/cm
2Having, is the above flux of 5 weight % if use the content of rare earth element again, then exists to produce the temperature that need be heated to more than 1500 ℃ in heating process, becomes more unfavorable.
(operation that is threaded of fixing body)
Secondly, the leading section 23a with fixing body 23 is threaded onto in the supported hole 25 that is mounted body 27.The periphery of this leading section 23a has been cut positive thread, and forms on the negative thread that can be threaded onto the supported hole 25 that is mounted body 27.Fixing body 23 is threaded, the grafting material in the front end face 23b contact supported hole 25 of leading section 23a.Like this, in the present embodiment, do not need fixing body 23 with respect to being mounted body 27 pressurizations.In addition, the average surface roughness of the leading section 23a of fixing body 23 is 0.4～1.6 μ m.
Have again, when being threaded, fixing body 23 coideals be the torque that applies 0.01～0.5Nm.Under the situation of the discontented 0.01Nm of torque, the possibility that exists crimp force deficiency and bond strength to descend.On the other hand, under the big situation of torque ratio 0.5Nm, the torque that produced of being threaded surpasses fixing body 23 or is mounted the strength of materials of body 27, has the possibility that deforms.
(heating process)
Under this state, with fixing body 23 and be mounted body 27 and be disposed in the inert gas environments such as nitrogen and argon gas or in the reduced pressure atmosphere, and heat with the junction temperature below 1500 ℃.In view of the above, good engagement state can be obtained, and the fixing body and the thermal distortion that is mounted body of nitrogen aluminium can be reduced with lower junction temperature.What junction temperature was better is 1400～1500 ℃.According to fixing body 23 and the size and the shape that are mounted body 27, it is desirable to keep 5 minutes～3 hours with the junction temperature below 1500 ℃.
In addition, it is desirable to rise to junction temperature for 0.5～10.0 ℃/minute with heat-up rate.In 0.5 ℃/timesharing of heat-up rate less than, flux crystallization and fusing point rise, and connectivity might variation.Surpassing 10.0 ℃/timesharing, may be in manufacturing process damaged, decrease in yield.
As mentioned above, the manufacture method according to the aluminum nitride bonded body of present embodiment with 1500 ℃ and following low junction temperature, can obtain good engagement state.Therefore, its engagement state of resulting aluminum nitride bonded body is good, and the distortion of aluminum nitride sintered product is little.And, because junction temperature is low, thus can reduce to engage institute's energy requirement, and the reworking after can not needing to engage, so can significantly reduce manufacturing cost.
Be described more specifically the present invention below by embodiment.
Embodiment 1
Embodiment 1 is described.At first, the aluminum nitride bonded body of example 1 of the present invention is described in detail.
(manufacturing process of aluminum nitride sintered product)
At first, in aluminium nitride powder 95 weight %, add yttrium oxide 5 weight %, and mix with ball mill as sintering aid.In resulting mixed powder, add caking agent, form particle by spray granulation.The resulting granules powder is configured as tabular molding and tubulose molding with metal die shaping and CIP.With resulting tabular molding (being mounted body) in nitrogen by pressure sintering 1860 ℃ of sintering 6 hours, tubulose molding (fixing body) is come with 1860 ℃ of sintering 6 hours by normal pressure-sintered in nitrogen.Fire by this hot pressing, above-mentioned tabular molding becomes tabular sintered body, and the tubulose molding becomes tubular body.
Secondly, on above-mentioned tabular sintered body, formed supported hole, formed positive thread at the leading section of tubulose molding with negative thread.This supported hole forms the leading section of the tubulose sintered compact that can be threaded.
(joint operation)
With calcium oxide (CaO) 50 weight % and aluminum oxide (Al
2O
3) flux that constituted of 50 weight % and the aluminium nitride powder that contains the yttrium (Y) of 5 weight % be mixed in PVA and the ethanol and make the pulpous state grafting material.In the bottom surface of the supported hole of above-mentioned tabular sintered body, evenly smear grafting material so that the amount of grafting material is 14mg/cm
2
Then, the leading section of tubular body is threaded onto in the supported hole of tabular sintered body front end face contact grafting material up to this leading section.Under this state, tubular body and tabular sintered body are disposed in the nitrogen, kept 2 hours down for 1450 ℃ at junction temperature.Heat-up rate is 3.3 ℃/minute, and nitrogen (pressure 1.5atm) is with 1200 ℃ of importings.Above operation is expressed as in table 1 " low temperature joint ".Have again, when being threaded the tubulose sintered compact, install, and be threaded into the bottom surface that the thrust that is produced pushes the supported hole of tabular sintered body with the front end of tubular body with the 0.1Nm torque.
Like this, by tubular body is joined on the tabular sintered body through knitting layer, and made aluminum nitride bonded body shown in Figure 2.
(evaluation method)
For the bonding part of the invention described above example 1 resulting aluminum nitride bonded body, valence and resistance to air loss.Intensity according to JIS R1601, is at room temperature measured four-point bending intensity.Intensity (is called " A-stage " in the following text) respectively before endurance test, measure after the endurance test.Endurance test is with making heat-up rate be 10 ℃/minute in atmosphere aluminum nitride bonded body to be heated to 800 ℃, and the processing of cool to room temperature repeats 100 times.
Resistance to air loss is, helium is imported from aluminum nitride bonded body is outside, and the leak volume that will flow into the helium in the pipe of tubular body from the junction surface measured with the helium leak detector.
These results represent in following table 1.
| Method of joining | No-load is arranged during joint | There is non-bolt at the junction surface | Initial stage (engaging the back) | Behind the thermal cycling test | The result | |||
| Intensity (Mpa) | Helium leak volume (TorrI/sec) | Intensity (Mpa) | Helium leak volume (TorrI/sec) | |||||
| Example 1 of the present invention | Low temperature engages | Do not have | Have | 280 | 1×10 -8Below | 275 | 1×10 -8Below | ○ |
| Comparative example 1 | Low temperature engages | Do not have | Do not have | 160 | 1×10 -8Below | 100 | 1×10 -8More than | △ |
| Comparative example 2 | Solid phase engages | Do not have | Have | 100 | 1×10 -8More than | 35 | 1×10 -8More than | × |
| Comparative example 3 | Liquid phase engages | Do not have | Have | 100 | 1×10 -8More than | 30 | 1×10 -8More than | × |
According to table 1, the aluminum nitride bonded body of example 1 of the present invention almost be can't see the decline of intensity behind thermal cycling test, and the spillage of helium is not confirmed to be yet and changes.
Comparative example
In addition, same with the invention described above example 1 in comparative example 1, be configured as tabular sintered body and tubular body, tubular body is joined on the tabular sintered body through knitting layer.But, at the leading section of tubular body, do not form positive thread, and do not form negative thread in the supported hole of tabular sintered body yet.
Have again, in comparative example 2,3, leading section in tubular body forms positive thread, in the supported hole of tabular sintered body, form negative thread, but, in comparative example 2, use solid phase to engage and be used as method of joining, in comparative example 3, use as a kind of solid-liquid in the liquid phase joint to engage.
Have again, in the solid phase of comparative example 2 engages, particularly, with 2.61 * 10
-4The yttrium nitrate solution hydrate Y (NO of mol/cc
3)
26H
2The O aqueous solution is applied on the junction surface, by be warmed up to 1850 ℃ and heat and engaged in two hours in nitrogen.
In addition, in the solid-liquid of comparative example 3 engages, particularly, with weight % with 37wt%CaO, 19wt%Y
2O
3, 44wt%Al
2O
3Blended mixed powder (1375 ℃ of ctystallizing points) is applied to this grafting material mixed ethanol on the junction surface as grafting material, by be warmed up to 1600 ℃ and heat and engaged in two hours in nitrogen.
Use the aluminum nitride bonded body of above comparative example 1～3, carry out intensity and the resistance to air loss evaluation same with example of the present invention 1.Its result represents in above-mentioned table 1.
From this table 1, judge, in comparative example 1～3, behind thermal cycling test, seen the decline of intensity, and confirm that the spillage of helium has also increased.
Like this, example of the present invention 1 and comparative example 1～3 are relatively confirmed aspect intensity behind thermal cycling test and the gas leakage favourable.
Embodiment 2
Then, embodiment 2 is described.This embodiment 2, with respect to embodiment 1, the flux that has only changed in the grafting material is formed, and other condition (for example the manufacture method of aluminum nitride bonded body etc.) is identical with embodiment 1.
The consisting of of flux makes calcium oxide and alumina powder become ratio of components as shown in following table 2.
Table 2
| Flux is formed | Knitting layer is formed | Bond strength (MPa) | ||||||
| CaO a great deal of (weight %) | Al 2O 3A great deal of (weight %) | Ca (weight %) | Al (weight %) | O (weight %) | N (weight %) | Y (weight %) | ||
| Example 2 of the | 41 | 59 | 7 | 52 | 13 | 25 | 3 | 295 |
| Example 3 of the present invention | 50 | 50 | 12 | 39 | 22 | 21 | 3 | 300 |
| Example 4 of the | 58 | 41 | 20 | 25 | 33 | 18 | 4 | 305 |
| Comparative example 4 | 68 | 32 | 23 | 17 | 33 | 24 | 3 | 230 |
| Comparative example 5 | 30 | 70 | 4 | 57 | 28 | 8 | 3 | 220 |
Above-mentioned flux and the alumina powder that contains 5 weight % yttriums (Y) be mixed in PVA and the ethanol and make the pulpous state grafting material.The ratio of mixture of flux and aluminium nitride powder is 60:40 with the weight ratio.Have, the applying amount of grafting material is all 14mg/cm again
2
Can judge that from table 2 aluminum nitride bonded body of example 2～4 of the present invention is than the bond strength height of comparative example 4,5.Have, the composition of the knitting layer of example 2～4 of the present invention is set at nitrogen 15～30 weight %, oxygen 10～35 weight %, aluminium 20～55 weight %, calcium 5～20 weight % again.In addition, the composition of the knitting layer of comparative example 4,5 is not in these scopes.
Embodiment 3
Then, embodiment 3 is described.This embodiment 3 with respect to embodiment 1, has only changed the front end face 23b shown in Figure 2 and the surfaceness of bottom surface 29, and other condition (for example the manufacture method of aluminum nitride bonded body etc.) is identical with embodiment 1.
Table 3
| The surface roughness Ra of | The surface roughness Ra of bottom surface 29 (μ m) | Bond strength (MPa) | |
| Example 5 of the present invention | 0.4 | 0.4 | 290 |
| Example 6 of the present invention | 1 | 1 | 280 |
| Example 7 of the present invention | 1.6 | 1.6 | 260 |
| Comparative example 6 | 0.3 | 0.4 | 230 |
| Comparative example 7 | 1.7 | 1.7 | 250 |
As shown in table 3, example 5～7 of the present invention, the average surface roughness of front end face 23b and bottom surface 29 is the scope of 0.4～1.6 μ m, average surface roughness is beyond the scope of 0.4～1.6 μ m in the comparative example 6,7.
Can judge that from table 3 bond strength of the aluminum nitride bonded body of example 5～7 of the present invention is than the bond strength height of comparative example 6,7.
Claims (6)
1. aluminum nitride bonded body is characterized in that possessing:
The bar-shaped fixing body that comprises aluminium nitride;
Comprise aluminium nitride, and the leading section of described fixing body is threaded onto the body that is mounted in the supported hole; And,
At these fixing bodies and being mounted in the contact part of body, be formed on fixing body at least and bear the pressure contact portion of crimp force by described being threaded, and with described fixing body be mounted the knitting layer that body engages,
This knitting layer comprises nitrogen, oxygen, aluminium, calcium, and the amount of rare earth element is discontented with 15 weight %.
2. aluminum nitride bonded body according to claim 1 is characterized in that,
Described knitting layer comprises 15～30 weight % nitrogen, 10～35 weight % oxygen, 20～55 weight % aluminium, 5～20 weight % calcium.
3. aluminum nitride bonded body according to claim 1 is characterized in that,
Described fixing body is formed inside has the cylindric of through hole, simultaneously, by described be mounted on the body to form be communicated to the patchhole of supported hole, and make the through hole of fixing body be communicated to described the inserting in the hole of body that be mounted.
4. the manufacture method of an aluminum nitride bonded body is characterized in that, has following steps:
In the bar-shaped fixing body that contains aluminium nitride and the step of smearing grafting material at least one of body that is mounted that contains aluminium nitride;
Described fixing body is threaded onto in the supported hole that is mounted body, and described fixing body is crimped onto the step that is mounted on the body by described grafting material; And,
By to described fixing body, grafting material and be mounted body and heat with the junction temperature below 1500 ℃, fixing body is bonded on the step that is mounted on the body by knitting layer,
Described grafting material contains calcium aluminium oxide or calcium oxide and aluminum oxide by comprising, and the flux and the aluminium nitride powder that contain the discontented 5 weight % of rare earth element, and with fixing body be mounted in the contact part of body and be bonded with each other by knitting layer because of the above-mentioned pressure contact portion that fixing body is born from the crimp force that is mounted body that is threaded at least.
5. the manufacture method of aluminum nitride bonded body according to claim 4 is characterized in that,
Described fixing body and being mounted in the contact part of body, the average surface roughness because of the described pressure contact portion that bears crimp force of being threaded is 0.4～1.6 μ m at least.
6. the manufacture method of aluminum nitride bonded body according to claim 4 is characterized in that,
Rise to described junction temperature for 0.5～10.0 ℃/minute with heat-up rate.
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|---|---|---|---|
| US75413705P | 2005-12-27 | 2005-12-27 | |
| US60/754,137 | 2005-12-27 |
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| US (1) | US20070144667A1 (en) |
| EP (1) | EP1803696B1 (en) |
| JP (2) | JP4921150B2 (en) |
| KR (1) | KR100847498B1 (en) |
| CN (1) | CN100506752C (en) |
| TW (1) | TWI308908B (en) |
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| CN114749754A (en) * | 2022-05-31 | 2022-07-15 | 核工业西南物理研究院 | Vacuum brazing evaluation test piece for vacuum brazing process evaluation |
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| US20090277388A1 (en) * | 2008-05-09 | 2009-11-12 | Applied Materials, Inc. | Heater with detachable shaft |
| US9624137B2 (en) * | 2011-11-30 | 2017-04-18 | Component Re-Engineering Company, Inc. | Low temperature method for hermetically joining non-diffusing ceramic materials |
| US9556074B2 (en) * | 2011-11-30 | 2017-01-31 | Component Re-Engineering Company, Inc. | Method for manufacture of a multi-layer plate device |
| US8932690B2 (en) * | 2011-11-30 | 2015-01-13 | Component Re-Engineering Company, Inc. | Plate and shaft device |
| EP3166909A1 (en) * | 2014-07-10 | 2017-05-17 | CeramTec GmbH | Laminated ceramic molded article having recesses |
| JP7569772B2 (en) * | 2021-10-07 | 2024-10-18 | 日本碍子株式会社 | Semiconductor manufacturing equipment parts |
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| JPH03279274A (en) * | 1990-03-28 | 1991-12-10 | Ngk Insulators Ltd | Joined ceramics |
| US5209525A (en) * | 1990-03-28 | 1993-05-11 | Ngk Insulators, Ltd. | Bonded ceramic structure |
| JP2783980B2 (en) * | 1994-09-01 | 1998-08-06 | 日本碍子株式会社 | Joint body and method of manufacturing the same |
| JP4070752B2 (en) * | 1997-01-30 | 2008-04-02 | 日本碍子株式会社 | Bonding agent for aluminum nitride ceramic substrate |
| JP3604888B2 (en) * | 1997-01-30 | 2004-12-22 | 日本碍子株式会社 | Jointed body of aluminum nitride-based ceramics substrate, method of manufacturing jointed body of aluminum nitride-based ceramics base, and bonding agent |
| JP2001342079A (en) * | 2000-05-30 | 2001-12-11 | Ibiden Co Ltd | Ceramic junction body |
| JP3966376B2 (en) * | 2001-09-11 | 2007-08-29 | 住友電気工業株式会社 | SUBSTRATE HOLDER, PROCESSING DEVICE, AND CERAMIC SUSCEPTOR FOR SEMICONDUCTOR MANUFACTURING DEVICE |
| WO2003077290A1 (en) * | 2002-03-13 | 2003-09-18 | Sumitomo Electric Industries, Ltd. | Holder for semiconductor production system |
| JP3520074B2 (en) * | 2002-03-28 | 2004-04-19 | 日本碍子株式会社 | Ceramic susceptor mounting structure, ceramic susceptor support structure, and ceramic susceptor support member |
| JP3832409B2 (en) * | 2002-09-18 | 2006-10-11 | 住友電気工業株式会社 | Wafer holder and semiconductor manufacturing apparatus |
| JP4787568B2 (en) * | 2004-11-16 | 2011-10-05 | 日本碍子株式会社 | Bonding agent, aluminum nitride bonded body, and manufacturing method thereof |
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| CN114749754A (en) * | 2022-05-31 | 2022-07-15 | 核工业西南物理研究院 | Vacuum brazing evaluation test piece for vacuum brazing process evaluation |
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| Publication number | Publication date |
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| CN100506752C (en) | 2009-07-01 |
| JP5367778B2 (en) | 2013-12-11 |
| TW200732272A (en) | 2007-09-01 |
| JP4921150B2 (en) | 2012-04-25 |
| TWI308908B (en) | 2009-04-21 |
| US20070144667A1 (en) | 2007-06-28 |
| JP2007176792A (en) | 2007-07-12 |
| JP2012031058A (en) | 2012-02-16 |
| KR100847498B1 (en) | 2008-07-22 |
| KR20070069030A (en) | 2007-07-02 |
| EP1803696A1 (en) | 2007-07-04 |
| EP1803696B1 (en) | 2012-10-24 |
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